CN101844222A - Controllable temperature gradient unidirectional solidification device and method - Google Patents
Controllable temperature gradient unidirectional solidification device and method Download PDFInfo
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- CN101844222A CN101844222A CN 201010194437 CN201010194437A CN101844222A CN 101844222 A CN101844222 A CN 101844222A CN 201010194437 CN201010194437 CN 201010194437 CN 201010194437 A CN201010194437 A CN 201010194437A CN 101844222 A CN101844222 A CN 101844222A
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Abstract
The invention belongs to the material preparation field, which provides a controllable temperature gradient unidirectional solidification device and a method and is applicable to the preparation of the material with magnetic anisotropy and structural anisotropy. The unidirectional solidification device consists of fusion, heat preservation, a pull-down mechanism, a cooling system and a control system. The fusion, unidirectional solidification and thermal processing are completed on the same device. By adjusting the relative position of a movable cooling ring (13) and a solid liquid interface, the temperature gradient of the solid liquid interface in the solidification process is controlled. The cooling ring and the solid liquid interface can be regulated and controlled at 10 to 200mm. The temperature gradient of the solid liquid interface can be regulated and controlled at 5 to 500 degrees centigrade/cm. The invention is applicable to the preparation of the rare earth giant magnetostrictive material, the Nd-Fe-B permanent magnet material and the samarium-cobalt permanent magnet material with magnetocrystalline anisotropy and the high temperature ally and steel material with the structural anisotropy. The invention has the advantages of stable technology, the good consistency of the prepared unidirectional solidification material and high finished product rate.
Description
Technical field
The invention belongs to field of material preparation, a kind of controllable temperature gradient unidirectional solidification device and method are provided, be applicable to that preparation has magnetic anisotropy and organizes anisotropic material.
Background technology
Directional solidification technique can provide the thermograde on the single direction in the metallic crystal process, eliminate the horizontal crystal boundary that generates in the crystallization process, makes crystal as far as possible along this direction growth, makes foundry goods have the column crystal or the single crystal organization structure of single direction.This characteristics of organizational structure can be strengthened physics or the mechanical performance on a certain direction of foundry goods, thereby in field of material preparation such as magnetic, high temperature alloy, iron and steel irreplaceable value is arranged.For example: rare earth ultra-magnetostriction material, Nd-Fe-Bo permanent magnet material, SmCo series permanent magnetic material with magnetocrystalline anisotropy, the ingot casting that utilizes directional solidification technique to make has the very high degree of orientation, make material along the directional solidification direction, be that magnetic property on the column crystal direction of growth is strengthened, obtain high-performance anisotropic magnetic material; Organize anisotropic material for having, as nickel base superalloy, cobalt base superalloy and ferrous materials, the columnar crystal structure of even tissue can improve its elevated temperature strength, creep resistant and unidirectional mechanical property.
Temperature gradient of solid-liquid interface has obvious influence to the tissue and the performance of material in the directional solidification process.Suitable, stable thermograde can guarantee evenly continuous growth of crystal in the directional solidification process, and then obtains the material of even tissue, excellent performance.And, by adjusting the material that thermograde can obtain required institutional framework and performance.The directional freeze method of open report and equipment do not relate to the control to temperature gradient of solid-liquid interface at present.A kind of apparatus for directional solidification that adopts drop-down cooling understructure is disclosed as U.S. Pat 5607007A1; U.S. Pat 6896030B2 and European patent EP 1321208A3 adopt the apparatus for directional solidification of similar structures to prepare the high-temperature alloy blades of complicated shape; Chinese patent 03156926 provides a kind of " one-step method " directional solidification processes and equipment that is used to prepare rare earth ultra-magnetostriction material; Chinese patent 2583113Y has invented a kind of device that is used to prepare single crystal super alloy directional solidification part; Chinese patent 93238966.X has introduced a kind of steel ingot directional solidification easy device.These method and apparatus can't be realized in the directional solidification process temperature gradient of solid-liquid interface being regulated and control, and the institutional framework and the consistency of performance of prepared material is poor, yield rate is lower.
Summary of the invention
At the problems referred to above, the present invention proposes a kind of controllable temperature gradient unidirectional solidification device and method, its objective is to realize the controlled of temperature gradient of solid-liquid interface in the directional solidification process, improves the uniformity and the finished material rate of unidirectional solidification material institutional framework and performance.
A kind of controllable temperature gradient unidirectional solidification device is characterized in that being made up of melting mechanism (1), heat preservation mechanism (2) and pull down mechanism (3); Melting mechanism (1) is by draw the cork running channel (9) formation of bar (6), bottom of the bell (5) on top and liftable molten metal temperature measuring mechanism (4), inner melting kettle (7) and induction coil (8) and cast; Heat preservation mechanism (2) insulation baffle plate (12) bottom mould (11) and mould outside graphite resistance heater (10) and heater is formed; Pull down mechanism (3) is by mould (11) outside removable water-cooling ring (13) and bottom cooling base (14) and control motor (15) formation.
The present invention is by adjusting the relative position of removable air ring (13) and solid liquid interface, temperature gradient of solid-liquid interface in the process of setting is controlled, air ring and solid liquid interface can be regulated and control at 10-200mm, temperature gradient of solid-liquid interface can be regulated and control at 5-500 ℃/cm, directional solidification speed 5-500mm/h; Melting, directional solidification, heat treatment are finished on an equipment.
The present invention includes following step:
1, cast is drawn the cork bar (6) inserts in the plug hole of melting kettle (7) bottom, and the directional solidification raw material that will have target component is then packed in the melting kettle (7) in the melting mechanism (1);
2, make device inside be in vacuum or inert gas shielding state;
3, start power supply the directional solidification raw material is carried out melting;
4, removable water-cooling ring (13) is transferred to desired location, start-up control motor (15) rises up into heat preservation mechanism with mould (11);
5, start heat preservation mechanism (2) interior graphite resistance heaters (10) power supply and heat, mould (11) temperature is reached more than the raw material fusing point;
6, promote after melting finishes and pour into a mould the bar (6) of drawing the cork, make molten metal enter mould (11) through running channel (9), start-up control motor (15) is along with moving down of cooling base (14) carried out directional solidification;
7, after mould (11) is all pulled out heat preservation mechanism (2), the temperature of heat preservation mechanism (2) is transferred to heat treatment temperature, unidirectional solidification material is risen in the heat preservation mechanism (2) again and carry out subsequent heat treatment, obtain unidirectional solidification material after the heat treatment.
The present invention is applicable to prepare to have rare earth ultra-magnetostriction material, Nd-Fe-Bo permanent magnet material, the SmCo series permanent magnetic material of magnetocrystalline anisotropy and have and organizes anisotropic high temperature alloy, ferrous materials.
Advantage of the present invention is:
The present invention passes through to adjust the control of the distance realization of removable air ring and solid liquid interface to temperature gradient of solid-liquid interface in the directional solidification process, and therefore, the present invention has the high advantage of unidirectional solidification material high conformity, yield rate of process stabilizing, preparation.The present invention is applicable to prepare to have rare earth ultra-magnetostriction material, Nd-Fe-Bo permanent magnet material, the SmCo series permanent magnetic material of magnetocrystalline anisotropy and have and organizes anisotropic high temperature alloy, ferrous materials by adjusting temperature gradient of solid-liquid interface.
Description of drawings
Fig. 1 is apparatus of the present invention schematic diagram.Label among the figure is: 1-melting mechanism; The 2-heat preservation mechanism; The 3-pull down mechanism; 4-liftable molten metal temperature measuring mechanism; The last bell of 5-; 6-pours into a mould the bar of drawing the cork; The 7-melting kettle; The 8-induction coil; The 9-running channel; 10-graphite resistance heater; The 11-mould; 12-is incubated baffle plate; The removable water-cooling ring of 13-; 14-cools off base; 15-controls motor.
The specific embodiment
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Tb, 99.5Dy and high-purity Fe by Tb
0.3Dy
0.7Fe
2(atomic ratio) 11.26kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1300 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1300 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to rare earth ultra-magnetostriction material.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures, and send rare earth ultra-magnetostriction material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, had at last<110〉orientation the rare earth ultra-magnetostriction material of even columnar crystal structure.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Tb, 99.5Dy and high-purity Fe by Tb
0.3Dy
0.7Fe
2(atomic ratio) 13.12kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1300 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1300 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification and all pull out heat preservation mechanism up to rare earth ultra-magnetostriction material.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures, and send rare earth ultra-magnetostriction material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, had at last<112〉orientation the rare earth ultra-magnetostriction material of even columnar crystal structure.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Tb, 99.5Dy and high-purity Fe by Tb
0.3Dy
0.7Fe
2(atomic ratio) 14.61kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1300 ℃.Removable water-cooling ring 13 is transferred to apart from 110mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 239.50 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1300 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 300mm/h to carry out directional solidification and all pull out heat preservation mechanism up to rare earth ultra-magnetostriction material.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures, and send rare earth ultra-magnetostriction material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, had at last<110+<112〉orientation the rare earth ultra-magnetostriction material of even columnar crystal structure.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Nd, high-purity Fe and B content and is 20% Fe-B alloy by Nd
13.5Fe
79.75B
6.75(atomic ratio) 12.63kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1400 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1400 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to Nd-Fe-Bo permanent magnet material.The temperature that reduces heat preservation mechanism 2 is to 900 ℃ of heat treatment temperatures, and sends Nd-Fe-Bo permanent magnet material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2h, obtains having at last the Nd-Fe-Bo permanent magnet material of even columnar crystal structure at last.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Nd, high-purity Fe and B content and is 20% Fe-B alloy by Nd
13.5Fe
79.75B
6.75(atomic ratio) 13.54kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1400 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1400 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification and all pull out heat preservation mechanism up to Nd-Fe-Bo permanent magnet material.The temperature that reduces heat preservation mechanism 2 is to 900 ℃ of heat treatment temperatures, and sends Nd-Fe-Bo permanent magnet material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2h, obtains having at last the Nd-Fe-Bo permanent magnet material of even columnar crystal structure at last.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Nd, high-purity Fe and B content and is 20% Fe-B alloy by Nd
13.5Fe
79.75B
6.75(atomic ratio) 10.18kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1400 ℃.Removable water-cooling ring 13 is transferred to apart from 70mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 343.70 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1400 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 200mm/h to carry out directional solidification and all pull out heat preservation mechanism up to Nd-Fe-Bo permanent magnet material.The temperature that reduces heat preservation mechanism 2 is to 900 ℃ of heat treatment temperatures, and sends Nd-Fe-Bo permanent magnet material back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2h, obtains having at last the Nd-Fe-Bo permanent magnet material of even columnar crystal structure at last.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by Sm
2Co
17(atomic ratio) 10.04kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1350 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1350 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification up to Sm
2Co
17Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 950 ℃ of heat treatment temperatures, and with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1h.With the speed of 500mm/h with Sm
2Co
17Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 600 ℃ of heat treatment temperatures, again with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2h.Obtain having the Sm of even columnar crystal structure at last
2Co
17Permanent-magnet material.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by Sm
2Co
17(atomic ratio) 14.15kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1350 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1350 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification up to Sm
2Co
17Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 950 ℃ of heat treatment temperatures, and with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1h.With the speed of 500mm/h with Sm
2Co
17Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 600 ℃ of heat treatment temperatures, again with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2h.Obtain having the Sm of even columnar crystal structure at last
2Co
17Permanent-magnet material.
Embodiment 9
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by Sm
2Co
17(atomic ratio) 12.27kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1350 ℃.Removable water-cooling ring 13 is transferred to apart from 90mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 291.60 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1350 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 270mm/h to carry out directional solidification up to Sm
2Co
17Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 950 ℃ of heat treatment temperatures, and with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1h.With the speed of 500mm/h with Sm
2Co
17Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 600 ℃ of heat treatment temperatures, again with Sm
2Co
17Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2h.Obtain having the Sm of even columnar crystal structure at last
2Co
17Permanent-magnet material.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by SmCo
5(atomic ratio) 13.04kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1390 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1390 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification up to SmCo
5Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 920 ℃ of heat treatment temperatures, and with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1.5h.With the speed of 500mm/h with SmCo
5Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 580 ℃ of heat treatment temperatures, again with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2.5h.Obtain having the SmCo of even columnar crystal structure at last
5Permanent-magnet material.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by SmCo
5(atomic ratio) 11.46kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1390 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1390 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification up to SmCo
5Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 920 ℃ of heat treatment temperatures, and with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1.5h.With the speed of 500mm/h with SmCo
5Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 580 ℃ of heat treatment temperatures, again with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2.5h.Obtain having the SmCo of even columnar crystal structure at last
5Permanent-magnet material.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, then purity is not less than 99.5%Sm and 99.5%Co by SmCo
5(atomic ratio) 12.72kg packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1390 ℃.Removable water-cooling ring 13 is transferred to apart from 160mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 109.25 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1390 ℃.The raw material refining back that finishes promotes the cast bar of drawing the cork, and molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, and start-up control motor 15 makes cooling base 14 move down with the speed of 310mm/h to carry out directional solidification up to SmCo
5Permanent-magnet material is all pulled out heat preservation mechanism.The temperature that reduces heat preservation mechanism 2 is to 920 ℃ of heat treatment temperatures, and with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 1.5h.With the speed of 500mm/h with SmCo
5Permanent-magnet material is pulled out heat preservation mechanism 2, and the temperature that reduces heat preservation mechanism 2 is to 580 ℃ of heat treatment temperatures, again with SmCo
5Permanent-magnet material is sent heat preservation mechanism back to the speed of 500mm/h and is heat-treated 2.5h.Obtain having the SmCo of even columnar crystal structure at last
5Permanent-magnet material.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.04, and B 0.005, and Cr 9.03, Co 4.52, and Al 5.5, and Mo 3.02, Nb 2.15, and W 3.22, and the surplus raw material 9.61kg of Ni packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1450 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to nickel base superalloy.The temperature that reduces heat preservation mechanism 2 is to 1220 ℃ of heat treatment temperatures and send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 3h.Speed with 500mm/h is pulled out heat preservation mechanism 2 with nickel base superalloy, and the temperature that reduces heat preservation mechanism 2 is sent nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treated 3h to 1050 ℃ of heat treatment temperatures.At last nickel base superalloy is pulled out heat preservation mechanism 2 with the speed of 500mm/h, the temperature that reduces heat preservation mechanism 2 is to 850 ℃ of heat treatment temperatures, send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treat 24h, stove is chilled to the nickel base superalloy that room temperature obtains having even columnar crystal structure.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.04, and B 0.005, and Cr 9.03, Co 4.52, and Al 5.5, and Mo 3.02, Nb 2.15, and W 3.22, and the surplus raw material 12.49kg of Ni packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1450 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification and all pull out heat preservation mechanism up to nickel base superalloy.The temperature that reduces heat preservation mechanism 2 is to 1220 ℃ of heat treatment temperatures and send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 3h.Speed with 500mm/h is pulled out heat preservation mechanism 2 with nickel base superalloy, and the temperature that reduces heat preservation mechanism 2 is sent nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treated 3h to 1050 ℃ of heat treatment temperatures.At last nickel base superalloy is pulled out heat preservation mechanism 2 with the speed of 500mm/h, the temperature that reduces heat preservation mechanism 2 is to 850 ℃ of heat treatment temperatures, send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treat 24h, stove is chilled to the nickel base superalloy that room temperature obtains having even columnar crystal structure.
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.04, and B 0.005, and Cr 9.03, Co 4.52, and Al 5.5, and Mo 3.02, Nb 2.15, and W 3.22, and the surplus raw material 15.62kg of Ni packs in the melting kettle 7.Start vacuum system vacuum is risen to 10W
-3A charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 140mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 161.35 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1450 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 180mm/h to carry out directional solidification and all pull out heat preservation mechanism up to nickel base superalloy.The temperature that reduces heat preservation mechanism 2 is to 1220 ℃ of heat treatment temperatures and send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 3h.Speed with 500mm/h is pulled out heat preservation mechanism 2 with nickel base superalloy, and the temperature that reduces heat preservation mechanism 2 is sent nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treated 3h to 1050 ℃ of heat treatment temperatures.At last nickel base superalloy is pulled out heat preservation mechanism 2 with the speed of 500mm/h, the temperature that reduces heat preservation mechanism 2 is to 850 ℃ of heat treatment temperatures, send nickel base superalloy back to heat preservation mechanism with the speed of 500mm/h again and heat-treat 24h, stove is chilled to the nickel base superalloy that room temperature obtains having even columnar crystal structure.
Embodiment 16
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.45, and Al 0.8, and Zr 0.15, and Ni 11, and Cr 25, and W 7.5, and Mo 0.2, and Ti 0.15, and the surplus raw material 9.39kg of Co packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1500 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1500 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to cobalt base superalloy.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures and send cobalt base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, obtains having the cobalt base superalloy of even columnar crystal structure at last.
Embodiment 17
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.45, and Al 0.8, and Zr 0.15, and Ni 11, and Cr 25, and W 7.5, and Mo 0.2, and Ti 0.15, and the surplus raw material 13.47kg of Co packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1500 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1500 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification and all pull out heat preservation mechanism up to cobalt base superalloy.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures and send cobalt base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, obtains having the cobalt base superalloy of even columnar crystal structure at last.
Embodiment 18
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: C 0.45, and Al 0.8, and Zr 0.15, and Ni 11, and Cr 25, and W 7.5, and Mo 0.2, and Ti 0.15, and the surplus raw material 15.36kg of Co packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1500 ℃.Removable water-cooling ring 13 is transferred to apart from 50mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 395.80 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1500 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 400mm/h to carry out directional solidification and all pull out heat preservation mechanism up to cobalt base superalloy.The temperature that reduces heat preservation mechanism 2 is to 800 ℃ of heat treatment temperatures and send cobalt base superalloy back to heat preservation mechanism with the speed of 500mm/h and heat-treat 2.5h, obtains having the cobalt base superalloy of even columnar crystal structure at last.
Embodiment 19
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: Si 0.29, Mn0.70, P0.03, S 0.02, and Cr 17.47, C 0.07, and Ni 9.27, and the 1Cr18Ni9Ti stainless steel raw material 15.33kg of Ti 0.06 packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 10mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 500 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1550 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to the 1Cr18Ni9Ti stainless steel material, promptly obtain having the 1Cr18Ni9Ti stainless steel material of even columnar crystal structure.
Embodiment 20
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, with composition (percentage by weight) be then: Si0.29, Mn 0.70, P 0.03, and S 0.02, and Cr 17.47, C0.07, Ni 9.27, and the 1Cr18Ni9Ti stainless steel raw material 13.57kg of Ti0.06 packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 200mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 5 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1550 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 5mm/h to carry out directional solidification and all pull out heat preservation mechanism up to the 1Cr18Ni9Ti stainless steel material, promptly obtain having the 1Cr18Ni9Ti stainless steel material of even columnar crystal structure.
Embodiment 21
Draw the cork bar 6 of cast is inserted in the plug hole of melting kettles 7 bottoms, and with composition (percentage by weight) be then: Si 0.29, Mn0.70, P 0.03, and S 0.02, and Cr 17.47, C 0.07, and Ni 9.27, and the 1Cr18Ni9Ti stainless steel raw material 13.68kg of Ti0.06 packs in the melting kettle 7.Start vacuum system vacuum is risen to 10
-3Pa charges into the argon gas of 0.5atm.Start power supply raw material is carried out heat fused, after raw material all melts, shake liftable temperature measuring mechanism handwheel and make thermometric bar contacting metal liquid carry out thermometric, and the adjustment inductive source power makes smelting temperature reach 1550 ℃.Removable water-cooling ring 13 is transferred to apart from 100mm place, directional solidification solid liquid interface lower end, make that temperature gradient of solid-liquid interface is 265.55 ℃/cm in the directional solidification process.Start-up control motor 15 rises to heat preservation mechanism 2 with mould 11, and starts cooling base and removable water-cooling ring recirculated water.Start heat preservation mechanism 2 interior graphite resistance heater 10 power supplys simultaneously and heat, make the temperature of mould 11 reach 1550 ℃.Promote after the raw material refining finishes and pour into a mould the bar of drawing the cork, molten metal is flowed down through running channel 9 cast from plug hole enter mould 11, start-up control motor 15 makes cooling base 14 move down with the speed of 500mm/h to carry out directional solidification and all pull out heat preservation mechanism up to the 1Cr18Ni9Ti stainless steel material, promptly obtain having the 1Cr18Ni9Ti stainless steel material of even columnar crystal structure.
Claims (4)
1. a controllable temperature gradient unidirectional solidification device is characterized in that being made up of melting mechanism (1), heat preservation mechanism (2) and pull down mechanism (3); Melting mechanism (1) is by draw the cork running channel (9) formation of bar (6), bottom of the bell (5) on top and liftable molten metal temperature measuring mechanism (4), inner melting kettle (7) and induction coil (8) and cast; Heat preservation mechanism (2) insulation baffle plate (12) bottom mould (11) and mould outside graphite resistance heater (10) and heater is formed; Pull down mechanism (3) is by mould (11) outside removable water-cooling ring (13) and bottom cooling base (14) and control motor (15) formation.
2. controllable temperature gradient unidirectional solidification method, it is characterized in that utilizing the described device for directionally solidifying of claim 1, by adjusting the relative position of removable air ring (13) and solid liquid interface, temperature gradient of solid-liquid interface in the process of setting is controlled, air ring and solid liquid interface can be regulated and control at 10-200mm, temperature gradient of solid-liquid interface can be regulated and control at 5-500 ℃/cm, directional solidification speed 5-500mm/h; Melting, directional solidification, heat treatment are finished on an equipment.
3. a kind of controllable temperature gradient unidirectional solidification method according to claim 2 is characterized in that comprising the steps:
1), the cast bar (6) of drawing the cork is inserted in the plug hole of melting kettle (7) bottom, the directional solidification raw material that will have target component is then packed in the melting kettle (7) in the melting mechanism (1);
2) make device inside be in vacuum or inert gas shielding state;
3), start power supply the directional solidification raw material is carried out melting;
4), removable water-cooling ring (13) is transferred to desired location, start-up control motor (15) rises up into heat preservation mechanism with mould (11);
5), start heat preservation mechanism (2) interior graphite resistance heaters (10) power supply and heat, mould (11) temperature is reached more than the raw material fusing point;
6), the melting back that finishes promotes the cast bar (6) of drawing the cork, and makes molten metal enter mould (11) through running channel (9), start-up control motor (15) is along with moving down of cooling base (14) carried out directional solidification;
7), after mould (11) is all pulled out heat preservation mechanism (2), the temperature of heat preservation mechanism (2) is transferred to heat treatment temperature, unidirectional solidification material is risen in the heat preservation mechanism (2) again and carries out subsequent heat treatment, obtain unidirectional solidification material after the heat treatment.
4. a kind of controllable temperature gradient unidirectional solidification method according to claim 2 is characterized in that this directional freeze method is applicable to that preparation has rare earth ultra-magnetostriction material, Nd-Fe-Bo permanent magnet material, the SmCo series permanent magnetic material of magnetocrystalline anisotropy and has to organize anisotropic high temperature alloy or have and organizes anisotropic ferrous materials.
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